银催化1-溴代炔烃的功能化反应:高区域和立体选择性合成(Z)-β-溴-1-芳基乙烯基芳基酯（英文）

发展一种银催化1-溴代炔烃的官能团反应,用于高度区域和立体选择性合成(Z)-β-溴-1-芳基乙烯基芳基酯.以市售的芳香羧酸为原料, Ag₂O为催化剂,以Et₃N为碱, 1-溴炔烃与芳香羧酸反应,高收率得到相应的(Z)-β-溴-1-芳基乙烯基芳基酯产物.研究结果表明, Ag₂O在反应中起着重要的催化作用.     

一锅法合成3-溴丙基乙酸酯

以1,3-丙二醇、氢溴酸（48％）和冰醋酸为原料,在带水剂的作用下,一锅法合成了3-溴丙基乙酸酯．考察了带水剂及追加醋酸或醋酸酐量对产率的影响,并通过气质联用仪对粗产品进行分析测定,推断其反应机理．结果表明：较适宜的合成条件为1,3-丙二醇0．21mol,1,3-丙二醇与氢溴酸（48％）、冰醋酸摩尔比为1：1：1．3,在带水剂甲苯（21mL）的作用下,反应2．5h,反应结束前1h追加4．8mL醋酸酐,合成效果最好,产率可达到95．7％．     

“一锅法”合成(E)-2-苯乙烯基喹啉-3,4-二酸二乙酯类衍生物（英文）

本文设计以2-溴甲基喹啉-3,4-二甲酸二乙酯为起始化合物,经一锅连续的Arbuzov反应/Horner-Wadsworth-Emmons(HWE)反应过程,简便而有效地合成了一系列结构新颖的(E)-2-苯乙烯基喹啉-3,4-二羧酸二乙酯类衍生物(3a～3i),其结构均已通过波谱数据和元素分析得以证实。     

4-(4-溴丁基)苯乙烯的合成

4-(4-溴丁基)苯乙烯的合成;溴丁基苯乙烯;对氯苯乙酮;对氯苯乙烯;合成     

无溶剂一锅法Al(ClO_4)_3催化合成α-氨基膦酸酯

以无水高氯酸铝为催化剂,将芳香醛、芳香胺及亚磷酸酯在无溶剂条件下一锅法反应,高效地合成了α-氨基膦酸酯,该催化剂优于其它已发现的催化剂[如Mg(ClO4)2,BiCl3,AlCl3等],建立了一种适用于含有钝化基团的芳香胺的α-氨基膦酸酯的新合成方法.     

一锅法合成2-硫脲嘧啶

采用一锅法合成了2-硫脲嘧啶,最佳反应条件为:硫脲33 mmol,n(乙酸乙酯)∶n(甲酸乙酯)∶n(甲醇钠)∶n(硫脲)=2.5∶2.0∶1.5∶1.0;乙酸乙酯与甲醇钠在甲苯(35 mL)中于80℃反应3 h;冷却后滴加甲酸乙酯,于25℃充分搅拌8 h后加入硫脲的乙醇(10 mL)溶液,回流反应3 h,收率54.7%。     

一锅法合成4-(5-芳基-1,3,4-噻二唑-2-氨甲基)苯酚衍生物

以2-氨基-5-芳基噻二唑衍生物和对羟基苯甲醛为原料,经亲核加成/脱水、还原两步一锅法合成了一系列新的4-(5-芳基-1,3,4-噻二唑-2-氨甲基)苯酚衍生物,反应具有时间短、后处理简单等优点.采用元素分析,NMR,IR以及质谱等多种谱学技术对产物进行了详细表征.     

乙二胺四乙酸四钠“一锅法”催化合成2-氨基-2-色烯衍生物

乙二胺四乙酸四钠能有效地催化芳香醛、丙二腈、1-萘酚在体积分数为95%乙醇介质中一锅法合成2-氨基-2-色烯衍生物. 该法具有催化剂价廉易得、反应条件温和、实验操作和后处理简便、收率高、催化剂能重复使用等优点.     

室温条件下硝酸铋高效催化“一锅法”合成4(3H)-喹唑啉酮衍生物

<正>4(3H)-喹唑啉酮及其衍生物具有抗疟疾、抗癌、抗痉挛、消炎、抗菌等多种生理活性[1-5]。因此,该类化合物的合成引起了人们极大的兴趣。1895年,Niementowski[6]发明了一种简单且易操作的合成4(3H)-喹唑啉酮的方法,该方法在1946年     

(Z)-2-(1H-咪唑-1-基)-1-(2,3,4-三甲氧基)苯乙酮肟酯的设计与合成

三甲基苯乙酮肟;立体异构体;(Z)-2-(1H-咪唑-1-基)-1-(2;3;4-三甲氧基)苯乙酮肟酯的设计与合成     

One-pot synthesis of(Z)-4-(2-bromovinyl)benezenesulfonamides by microwave-induced simultaneous debrominative decarboxylation and sulfamation of anti-2,3-dibromo-3-(4-chlorosulfonylphenyl)propanoic acid

One-pot simultaneous debrominative decarboxylation and sulfamation of anti-2,3-dibromo-3-(4-chlorosulfonylphenyl)propa-noic acid in DMF (for alkyl amines) or DMF-pyridine (for aryl amines) using a diverse range of alkyl and aryl amines under microwave irradiation condition stereoselectively afforded (Z)-4-(2-bromovinyl)benzenesulfonamides in good yields.     

One-pot synthesis of (Z)-4-(2-bromovinyl)benezenesulfonamides by microwave-induced simultaneous debrominative decarboxylation and sulfamation of anti-2,3-dibromo-3-(4-hlorosulfonylphenyl)propanoic acid

One-pot simultaneous debrominative decarboxylation and sulfamation of anti-2,3-dibromo-3-(4-chlorosulfonylphenyl)propanoic acid in DMF (for alkyl amines) or DMF-pyridine (for aryl amines) using a diverse range of alkyl and aryl amines under microwave irradiation condition stereoselectively afforded (Z)-4-(2-bromovinyl)benzenesulfonamides in good yields.     

4-(5-aryl-2-oxazolyl)benzenesulfonic acid derivatives containing a dimethylamino group

Condensation of 4-chlorosulfonyl- and 4-fluorosulfonyl-benzoyl chlorides with p-dimethylamino--aminoacetophenone followed by cyclodehydration of the resulting amides leads to the formation of 4-(5-dimethylaminophenyl-2-oxazolyl)benzenesulfonyl halides, and the corresponding sulfonic ester, sulfomorpholide, sulfonamide, and sodium salt are synthesized from them. The spectral and luminescence properties of the compounds synthesized have been studied in toluene, ethanol, and DMF. The ability of the sulfonyl group to transmit the electronic effects of the substituents on it to the overall molecular -electron system of 2,5-diaryloxazole has been demonstrated. Salvation fluorochromia has been detected in polar solvents. In some of the compounds studied the Stokes shift exceeds 200 nm.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 2, pp. 234–237, February, 1993.     

Convenient one-pot synthesis of functionalized （E）-2-arylvinyl bromides from （E）-4-（2-bromovinyl）phenyl acetate

A convenient one-pot synthesis of functionalized (E)-2-arylvinyl bromides was achieved by microwave-induced deacetylation and subsequent acylation using dicyclohexyl carbodiimide (DCC) and dimethylamino-pyridine (DMAP) at room temperature from (E)-4-(2-bromovinyl)phenyl acetate.     

One-pot synthesis of 3-(2-cyanophenyl)quinazolin-4(3H)-one

Anthranilonitrile reacting with formic acid at room temperature for three days gave 64% of 3-(2-cyanophenyl)quinazolin-4(3H)-one. Under similar conditions anthranilic acid. 4-nitroaniline, and 2,5-dichloroaniline were N-formylated in good yields.Institute of Organic Chemistry and Technology, Silesian Technical University, Krzywoustego, 4, 44–100 Gliwice, Poland; e-mail: wojtex@zeus.polsl.gliwice.pl. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 7, pp. 922–924, July, 2000.     

The synthesis of (Z)-2-(5-amino-1,2,4-thiadiazol-3-yl)-2-ethoxyiminoacetic acid

The objective was to synthesize (Z)-2-(5-Amino-1,2,4-thiadiazol-3-yl)-2-ethoxyiminoacetic acid (the side chain for Ceftaroline fosamil). Oximation and alkylation were used on cyanoacetamide to get 2-cyano-2-hydroxyiminoacetamide, which became 2-ethyoxyiminopropanedinitrile through reaction with phosphorus oxychloride, and then aminolysis to get 2-ethoxyiminopropanedinitrile, which became 2-ethoxyimion-2-(5-amino-1,2,4 thiadiazol-3-yl) acetonitrile by brominating and with KSCN, followed by hydrolysis to get (Z)-2-(5-Amino-1,2,4-thiadiazol-3-yl)-2-ethoxyiminoacetic acid.     

Synthesis of (Z)-4-hydroxytamoxifen and (Z)-2-[4-[1-(p-hydroxyphenyl)-2-phenyl]-1butenyl]phenoxyacetic acid

The synthesis of (Z)-4-hydroxytamoxifen and (Z)-2-[4-[1-(p-hydroxyphenyl)-2-phenyl]-1-butenyl]phenoxyacetic acid was accomplished using a McMurry reaction as the key step. The perfluorotolyl derivatives of the McMurry products enabled the separation of the minor undesirable geometrical isomer. The methodology proceeds without E,Z isomerization, employs a very mild final debenzylation step compatible with a large array of functional groups, and can be applied to the generation of a variety of 4-hydroxytamoxifen analogues.